接枝中空纤维膜过滤-液相色谱/串联质谱法检测血浆中盐酸克伦特罗  

Analysis of clenbuterol in plasma by grafted hollow fiber membrane filtration-HPLC-Tandem mass spectrometry

作　　者：王宛[1,2] 覃素姿 李林森[2] 魏俊富[3] 

机构地区：[1]天津工业大学材料科学与工程学院,天津300387 [2]天津博纳艾杰尔科技有限公司,天津300462 [3]天津工业大学环境与化学工程学院,天津300387

出　　处：《分析试验室》2015年第3期263-266,共4页Chinese Journal of Analysis Laboratory

基　　金：国家高技术研究发展计划(2013AA065600);国家科技支撑计划项目(2012BAK25B00)资助

摘　　要：建立了接枝改性的中空纤维膜过滤法净化处理-液相色谱-串联质谱法（LC-MS/MS）测定血浆中痕量盐酸克伦特罗的方法。血浆样品经改性中空纤维膜的过滤,通过膜上接枝的离子交换基团的吸附作用和膜孔的超滤作用去除其中的磷脂和蛋白质,消除了基质效应,提高了LC-MS/MS检测盐酸克伦特罗的灵敏度。色谱条件为：色谱柱采用Venusil MP C18（2.1×50 mm,3μm,10 nm）,流动相为乙腈/0.1%甲酸水溶液（15：85,V/V）,流速为200μL/min,柱温30℃,进样量5μL。质谱模式为电喷雾电离正模式。在1~100 ng/m L范围内,线性关系良好;检出限为0.21 ng/m L,回收率在90%~105%之间,RSD为3.8%~9.1%。方法适合血浆样品中痕量盐酸克伦特罗的检测。This article introduces a novel sample treatment using functional hollow fiber membrane in the analysis of clenbuterol from plasma. In order to eliminate the matrix effect caused by impurities,such as protein and phospholipid,plasma sample was filtered by a hollow fiber ultra filtration membrane with carboxyl functional group in the pore. Then the filtered sample was analysed on a reversed-phase C18 column using acetonitrile /0. 1% formic acid in water（ 15∶ 85,V / V） as the mobile phase and measured by tandem mass spectrometer in the positive mode of electric spray ionization. The calibration curves obtained for studied drugs show reasonable linearity（ r 〉 0. 9998） in the range from 1 ng / m L to 100 ng / m L. The limit of detection（ LOD） is0. 21 ng / m L. The relative standard deviations（ RSDs） of the method are investigated at four concentrations（ 2,5,10 and 20 ng / m L） and are in the range of 3. 8% ~ 9. 1%（ n = 6）. Finally,the proposed method has been effectively employed in extraction and determination of the drugs in biological samples.

关 键 词：接枝中空纤维膜 液相色谱-串联质谱法 血浆 盐酸克伦特罗 

分 类 号：O657.63[理学—分析化学]